HuagongsheHuagongshe Chemistry Print Report · For research reference only
4-Chloroaniline → 2-chloro-N-(4-chlorophenyl)-6-phenylpyrimidin-4-amine
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | 4-Chloroaniline | HCID 7812 | — |
| Reactant | Lithium diisopropylamide | HCID 2724682 | — |
| Reactant | Ethyl acetate hexane | HCID 21226206 | — |
| Reactant | 2,4-Dichloro-6-(2-chloro-6-fluorophenyl)pyrimidine | HCID 86661471 | — |
| Solvent | Tetrahydrofuran | HCID 8028 | — |
| Product | 2-chloro-N-(4-chlorophenyl)-6-phenylpyrimidin-4-amine | HCID 86661473 | — |
Reaction Steps
To 1 mmol of 2,4-dichloro-6-phenylpyrimidine (X) and 4-chloroaniline in 4 mL of dry THF was added 1 mmol (0.5 mL, 2M in THF/heptane/ethylbenzene) of lithium diisopropylamide. The reaction was followed by TLC (30% ethyl acetate/hexane). The reaction mixture was partitioned between ethyl acetate and saturated aqueous sodium bicarbonate and the organic layers were dried over magnesium sulfate and concentrated under reduced pressure. The mixture was purified by chromatography on silica gel with elution by 30% ethyl acetate/hexanes to afford 70 mg of 2-chloro-N-(4-chlorophenyl)-6-phenylpyrimidin-4-amine (XII) as an amorphous solid. ESI/MS 315.883, 317.915 (M+H).
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US09321735B2 |
| Source dataset | uspto-grants-2016_04 |
| ORD ID | ord-6b8475bc4b2b4e19a593f89947000524 |
| Source note | uspto-grants-2016_04 |